Method of preparing low-molecular-weight styrene-acrylate emulsion copolymer

A technology of acrylate and emulsion copolymerization, which is applied in the fields of instruments, optics, electrography, etc., can solve the problems of high equipment cost, high energy consumption and high manufacturing cost, and achieve the effect of reducing mercaptan content, simple operation and good effect.

Active Publication Date: 2014-04-02
EAST CHINA UNIV OF SCI & TECH +1
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Problems solved by technology

For example, Chinese patent (publication number CN101240046A) discloses a method for preparing brominated polystyrene with low molecular weight and narrow distribution by living / controllable polymerization, using atom transfer radical polymerization (ATRP) or reverse atom transfer radical polymerization (FATRP ) technology to prepare low-molecular-weight polymers, which have the advantages of high controllability of the molecular structure of the product and narrow molecular weight distribution, but the reaction conditions are fine and harsh, and the manufacturing cost is high, which is not suitable for large-scale industrial production; US patent (US4314044A) discloses an improved The method of controlling the molecular weight of the product by the amount of initiator and metal ion compound, wherein the amount of initiator is as high as 3.5% of the total amount of monomers. The limitation of this technology is that on the one hand, a large amount of initiator makes the end of the polymer molecule have ionic groups , easy to change the properties of the polymer, and on the other hand, metal ions are easy to affect the color of the product; European Patent (Patent No. 1,274,942, published on October 2, 1990) discloses a free radical polymerization of acrylic acid in supercritical carbon dioxide at 80°C method, but the exothermic temperature reaches 146°C during the reaction process, which easily leads to product deterioration; Chinese patent (authorized announcement number CN105413) discloses a preparation method with low molecular weight (number average molecular weight as low as 5000), that is, the polymerization reaction occurs at a high temperature Carried out in supercritical carbon dioxide at 200°C and pressure higher than 3500Psi, there are problems such as high equipment cost and large energy consumption

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  • Method of preparing low-molecular-weight styrene-acrylate emulsion copolymer

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Experimental program
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Effect test

Embodiment 1

[0026] In a 5000ml four-neck reaction flask equipped with a stirring motor, reflux condenser, thermometer and dropping funnel, add 1820ml deionized water, 15.0g lauryl polyoxyethylene (10) ether acetic acid, adjust the pH value to 8.0 with ammonia water, add 135.0g styrene, 40.4g butyl acrylate, 3.6g hydroxyethyl methacrylate, 1.0g acrylic acid and 3.6g n-dodecanethiol, start stirring, heat the mixture to 85°C, add 15.0g concentration of 10% Aqueous ammonium persulfate solution was reacted for 1 hour to prepare seed emulsion. Then 1215.0g of styrene, 363.6g of butyl acrylate, 32.4g of hydroxyethyl methacrylate, 9.0g of acrylic acid and 32.4g of n-dodecanethiol were mixed evenly, and another 35.0g of lauryl polyoxyethylene (10) ether acetic acid Dissolve in 700ml of deionized water, adjust the pH value to 8.0 with ammonia water, add 225g of 5% ammonium persulfate aqueous solution, and stir the above-mentioned monomer, chain transfer agent, emulsifier and initiator aqueous solut...

Embodiment 2

[0030] In a 5000ml four-neck reaction flask equipped with a stirring motor, reflux condenser, thermometer and dropping funnel, add 1820ml deionized water, 15.0g lauryl polyoxyethylene (10) ether acetic acid, adjust the pH value to 8.0 with ammonia water, add 135.0g styrene, 40.4g butyl acrylate, 3.6g hydroxyethyl methacrylate, 1.0g acrylic acid, 0.6g n-dodecanethiol, 7.2g carbon tetrachloride, start stirring, heat the mixture to 85°C, add 15.0 g of a 10% ammonium persulfate aqueous solution was reacted for 1 hour to prepare a seed emulsion. Then 1215.0g styrene, 363.6g butyl acrylate, 32.4g hydroxyethyl methacrylate, 9.0g acrylic acid, 5.4g n-dodecanethiol, 64.8g carbon tetrachloride were mixed evenly, and another 35.0g lauryl alcohol Dissolve oxyethylene (10) ether acetic acid in 700ml of deionized water, adjust the pH value to 8.0 with ammonia water, add 225g of 5% ammonium persulfate aqueous solution, and stir the above monomer, chain transfer agent, emulsifier and initiato...

Embodiment 3

[0035] In a 5000ml four-neck reaction flask equipped with a stirring motor, reflux condenser, thermometer and dropping funnel, add 1820ml deionized water, 15.0g lauryl polyoxyethylene (10) ether acetic acid, adjust the pH value to 8.0 with ammonia water, add 135.0g styrene, 40.4g butyl acrylate, 3.6g hydroxyethyl methacrylate, 1.0g acrylic acid and 18g carbon tetrachloride, start stirring, heat the mixture to 85°C, add 15.0g concentration of 10% persulfuric acid Ammonium aqueous solution was reacted for 1 hour to prepare a seed emulsion. Then 1215.0g styrene, 363.6g butyl acrylate, 32.4g hydroxyethyl methacrylate, 9.0g acrylic acid and 162g carbon tetrachloride were mixed evenly, and 35.0g lauryl polyoxyethylene (10) ether acetic acid was dissolved in In 700ml of deionized water, adjust the pH value to 8.0 with ammonia water, add 225g of 5% ammonium persulfate aqueous solution, and stir the above-mentioned monomer, chain transfer agent, emulsifier and initiator aqueous solutio...

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Abstract

The invention relates to a method of preparing low-molecular-weight styrene-acrylate emulsion copolymer, and the method is designed so as to solve technical problems of fine and harsh reaction conditions, high manufacturing costs, relatively large energy consumption and environment pollution, and poor polymer stability existing in present method. The method uses a semi-continuous emulsion polymerization method, and main design points are that employed chain transferring agent comprises thiols and halogenated hydrocarbons. The method comprises: (1) preparing a seed emulsion, (2) preparing a pre-emulsion, (3) uniformly adding the pre-emulsion into the seed emulsion, and controlling a reaction time and temperature; (4) distilling under a reduced pressure after the polymerization reaction, thereby distilling the halogenated hydrocarbons and volatile components and preparing the low-molecular-weight emulsion copolymer. The method is simple to operate, low in cost and good in effect, reduces mercaptan contents containing offensive odor during a preparation process, thereby the synthesized product being environmental-friendly, non-polluted, and wide in application range, and the method is suitable for being used as the method for the low-molecular-weight emulsion copolymer, or improvement of similar methods.

Description

technical field [0001] The invention relates to a method for preparing low-molecular-weight styrene-acrylate emulsion copolymer for laser printer or copier toner. Background technique [0002] Low-molecular-weight copolymer resins are widely used in the toner field. Toners with low-molecular-weight resins as binders can reduce melt viscosity and increase fusing strength, thereby improving image clarity and resolution. Low-molecular-weight resins can also reduce the melting temperature of toner, improve low-temperature fixing effects, and meet high-performance printing requirements while reducing energy consumption. [0003] Usually, the most commonly used method for synthesizing low-molecular-weight polymers in emulsion polymerization is to add thiol compounds, which have a high chain transfer constant and have a significant effect on reducing molecular weight. But the disadvantage is that the product smells bad and pollutes the environment; and because of its high boiling...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F212/08C08F220/18C08F220/28C08F220/06C08F2/38G03G9/08
Inventor 吴国章管爱国李保文
Owner EAST CHINA UNIV OF SCI & TECH
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